We synthesized Nanocrystalline nickel ferrite powder using co-precipitation method and studied the effect of sintering at 100, 400, 600, 800 °C on the prepared samples. X-ray diffraction (XRD) and transmission electron microscopy (TEM) were used to characterize the samples. XRD patterns show crystalline nature of the sample and the spinel structure of NiFe2O4. Particle size and morphology of the nanocrystalline powders were determined by TEM. The average particle sizes were identified to be 10 nm. Results indicate that the chemical synthesis by co-precipitation method leads to obtain nano crystalline nickel ferrite with controllable particle size.
When you are citing the document, use the following link http://essuir.sumdu.edu.ua/handle/123456789/3582

Emdadul, Islam S.K.

Sharma, Pankaj

SocioEconomic Challenges Journal (Sumy State University)

JOURNAL OF NANO- AND ELECTRONIC PHYSICS  ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ 
Vol. 6 No 1, 01008(4pp) (2014) Том 6 № 1, 01008(4cc) (2014) 
 
 
2077-6772/2014/6(1)01008(4) 01008-1  2014 Sumy State University 
 
Synthesis and Characterization of Nickel Ferrite: Role of Sintering Temperature on  
Structural Parameters 
 
S.K. Emdadul Islam, Pankaj Sharma* 
 
Department of Physics and Materials Science, Jaypee University of Information Technology,  
Waknaghat, Solan, H.P. (173234) India 
 
 (Received 30 October 2013; revised manuscript received 04 April 2014; published online 06 April 2014) 
 
We synthesized Nanocrystalline nickel ferrite powder using co-precipitation method and studied the ef-
fect of sintering at 100, 400, 600, 800 C on the prepared samples. X-ray diffraction (XRD) and transmis-
sion electron microscopy (TEM) were used to characterize the samples. XRD patterns show crystalline na-
ture of the sample and the spinel structure of NiFe2O4. Particle size and morphology of the nanocrystalline 
powders were determined by TEM. The average particle sizes were identified to be 10 nm. Results indicate 
that the chemical synthesis by co-precipitation method leads to obtain nano crystalline nickel ferrite with 
controllable particle size. 
 
Keywords: Co-precipitation, Ferrites, Structural parameters. 
 
 PACS numbers: 75.50.Gg, 73.63.Bd 
 
 
                                                          
* pks_phy@yahoo.co.in 
1. INTRODUCTION 
 
Magnetic nanopowders of spinel ferrites (MFe2O4, 
M  Ni, Co, Mn, Zn etc) are one of the important mate-
rials which was first synthesized about 50 years ago [1] 
and it has got high attention  since few decades due to 
their useful electromagnetic characteristics for a huge 
number of technological applications such as infor-
mation storage system, radio frequency coils, trans-
former, medical field for MRI, sensor, as radar absorb-
ing materials (RAM) in military to increase the invisibil-
ity to radar etc [2-9]. This is mainly due to their proper-
ties are vastly differ from the corresponding bulk mate-
rial. The function of these bulk ferrite materials is lim-
ited to a few megahertz frequency due to high electrical 
conductivity and domain wall resonance [10-11]. But in 
recent time’s electronic industry demand more compact 
cores for work at higher frequency [12]. This problem of 
domain wall resonance could be avoided by synthesizing 
ferrite nanoparticles. In this case domain formation is not 
favorable energetically below a critical dimension of the 
particle and it exists as a single domain [13]. Ferrite na-
noparticles can be synthesized by wet chemical method 
such as co-precipitation [14], sol-gel [15], reverse micelles 
[16], polymeric precursor  and hydrothermal process [17-
18]. The formula of the cubic structure of spinel ferrites 
are described as [A][B]2O4, where A is the tetrahedral and 
B is octahedral cation sites, in a FCC anion (oxygen) sub-
lattice. NiFe2O4 has a normal spinel structure with Ni2 + 
ions in the A-site and Fe3+ ions in the B-sites [19].  
In the present work, we have used the co-precipitation 
method due to its low cost, tailor made synthesis condi-
tions and is very simple method to provide homogeneous 
powders in greater amount at temperature close to 60 C 
[20]. Several preparation conditions such as concentration, 
molar ratio of the cation, pH of the solution and tempera-
ture can have an impact on the particle size of the ferrites 
and their properties [21]. NiFe2O4 powders are sintered at 
different temperatures. The lattice constant, crystal 
strain, dislocation density, phase of the ferrites and struc-
tural morphology of the nanocrystalline powders were 
studied. 
2. EXPERIMENTAL DETAILS 
 
2.1 Chemicals 
 
Nickel chloride (NiCI2.6H2O); anhydrous ferric chlo-
ride (FeCl3); Sodium Hydroxide (NaOH). All chemical 
were purchased from Merck (AR Grade) and used with-
out further purification.  
 
2.2 Synthesis 
 
Nickel ferrite powders with compositions NiFe2O4 
have been synthesized via co-precipitation method. First-
ly, 0.5M NiCl2.6H20 solution is made by adding 11.88g in 
100ml of double distilled water, simultaneously, 1M an-
hydrous FeCl3 solution is made by adding 16.22 g in 100 
ml of double distilled water. 0.4N NaOH solution (4 g 
NaOH pallet in 250 ml of distilled water) is used as pre-
cipitating agent. 50 ml of nickel chloride solution and 
50 ml of ferric chloride solution were mixed and kept at 
60 C for 30 minutes. In this mixture, added the boiling 
NaOH solution under constant stirring till the pH of the 
solution becomes 12. Nanoferrites are formed by conver-
sion of metal salts into hydroxides, followed by transfor-
mation of hydroxides into ferrites. The final solution was 
maintained at 85 C for 80 minutes, this time is sufficient 
for the transformation of hydroxides into spinel ferrite. 
Particles were filtered from the solution and were washed 
several times with double distilled water. Collected parti-
cle were then dried at 80 C. The samples were then 
grinded using mortar pestle and sintered at 100 C, 
400 C, 600 C and 800 C for 4 hrs. The precipitated fer-
rite is chocolate brown in colour. The overall chemical 
reaction for the formation of NiFe2O4 may be written by 
the following way [22-23]: 
 
Ni2 + + 2Fe3 + + 8OH –                   NiFe2O4 + 4H2O 
 
2.3 Characterization 
 
The phase identification of the synthesized powder 
sample of NiFe2O4 was done by using X-ray diffractom-
 PANKAJ SHARMA, S.K. EMDADUL ISLAM J. NANO- ELECTRON PHYS. 6, 01008 (2014) 
 
 
01008-2 
eter (XRD) having Cu-Ka radiation. Goniome-
ter  PW3050 / 60 (Theta / Theta); Minimum step size 
2θ: 0.001; Minimum step size Omega: 0.001. The struc-
tural morphology is investigated using transmission 
electron microscopy (TEM)[Hitachi, H-7500, 40-120 kV 
operating voltage] at 90 kV. 
 
3. RESULTS AND DISCUSSION 
 
Fig. (1-4) shows the XRD patterns of powder sam-
ples after sintering at different temperatures 100 C, 
400 C, 600 C and 800 C respectively. XRD data have 
been used to calculate structural parameters grain size, 
lattice parameter, strain of the crystal and dislocation 
density of the prepared sample. The average particle 
size of the sample was calculated by using Scherrer’s 
formula [26]: 
 
 D  0.9 / cos (1) 
 
where  is full width at half maxima and  is Bragg’s 
angle. 
The average strain (Є) of the sample was calculated 
by Stokes Wilson equation [25]: 
 
 Є  /4tan  (2) 
 
Equation is used to calculate the dislocation density [27], 
 
 δ  15ε / aD  (3) 
 
where D is average grain size, a is lattice parameter[27] 
 
 a  d  (h2 + k2 + l2)0.5 (4) 
 
where d is spacing between two planes. 
The values of parameters mentioned above are 
shown in Table 1. With increasing sintering temperature 
up to 600 C crystal strain and dislocation density de-
creases due to an increase in particle size, but at 800 C 
these parameters increases and particle size decreases. 
These changes in grain size, crystal strain and disloca-
tion density may be due to the crystal deformation after 
certain temperature. Lattice parameter of the prepared 
sample decreases with increasing sintering temperature 
this is may be due to compactness of the lattice in the 
crystal increases. 
 
10 20 30 40 50 60 70 80
0
20
40
60
80
100
120
140
160
180
200
in
te
n
s
it
y
2 theta(deg)
(311)
(222)
(400) (440)
 
 
Fig. 1 – XRD Pattern for NiFe2O4 at a sintering temperature 
of 100 C 
10 20 30 40 50 60 70 80
0
20
40
60
In
te
n
s
it
y
/a
.u
400
311
440
622
2 Theta(Deg)  
 
Fig. 2 – XRD Pattern for NiFe2O4 at a sintering temperature 
of 400 C 
 
10 20 30 40 50 60 70 80 90
0
100
200
300
400
500
in
te
n
s
it
y
2 theta(deg)
(220)
(311)
(222)
(400)
(511)
(440)
(5330
 
 
Fig. 3 – XRD Pattern for NiFe2O4 at a sintering temperature 
of 600 C 
 
10 20 30 40 50 60 70 80
-100
0
100
200
300
400
500
600
700
in
te
n
s
it
y
2 theta(deg)
(311)
(220)
(400)
(222)
(422)
(511)
(440)
(533)
 
 
Fig. 4 – XRD Pattern for NiFe2O4 at a sintering temperature 
of 800 C 
 
The characteristic peaks of NiFe2O4 from figure 1-4 
confirm the spinel structure of the powder sample and 
changes phase at different sintering temperature. The 
reflection peaks for 100 C are corresponding to (311), 
(222), (400), (440) planes, for 400 C the planes are 
(311), (400), (440) and (622)  and for 600 C and 800 C 
planes are (220), (311), (222), (400), (511), (440) and 
(533) [24]. At 100 C all the characteristic peaks are not 
intense, two broad lightly intense peaks for (311) and 
(222) plane are observed. Peak corresponding to (400)  
 
 SYNTHESIS AND CHARACTERIZATION OF NICKEL FERRITE… J. NANO- ELECTRON PHYS. 6, 01008 (2014) 
 
 
01008-3 
 
 
Fig. 5 – TEM Images for NiFe2O4 at a sintering temperature of 100 C 
 
 
 
Fig. 6 – TEM Images for NiFe2O4 at a sintering temperature of 800 C 
 
Table 1 – Lattice Parameter, Strain and Dislocation Density for NiFe2O4 at a sintering temperature of 100, 400, 600 and 800 C 
 
Sintering 
Temperature 
(C) 
Lattice parame-
ter (a) 
(Å) 
Crystal 
Strain (Є) 
Dislocation 
Density (δ) 
Particle size (D) 
(nm) 
100 8.3857 6.60  10 – 4 4.5  1014 26 
400 8.3354 5.68  10 – 4 2.7  1014 37 
600 8.3540 5.18  10 – 4 2.3  1014 42 
800 8.3253 8.28  10 – 4 5.3  1014 28 
 
plane is more intense for sintering temperature 400 C 
in comparison to 100 C. For sintering temperature 
600 C, sharp and more intense peaks are obtained for 
(400) plane along with (220), (511), and (533) planes. 
Comparing figures (1-4) all peaks become more intense 
and sharp with increasing sintering temperature i.e., 
crystalline nature is increased. Since plane (400) has 
same intensity for sintering temperature 400 C and 
600 C so confirms that the phase of the powder crystal 
is same. But ≥ 600 C highly intense characteristic peaks 
 PANKAJ SHARMA, S.K. EMDADUL ISLAM J. NANO- ELECTRON PHYS. 6, 01008 (2014) 
 
 
01008-4 
for (311) plane is found. It shows that phase changes 
above 600 C sintering temperature and also with in-
creasing the sintering temperature leads to higher crys-
tallinity. 
The TEM micrographs for NiFe2O4 powder are shown 
in fig. (5-6). The morphology of the prepared sample is 
mostly cubical with some agglomeration. The average 
particle size is estimated to about 10 nm for powder sin-
tered at temperatures 100, 400, 600 and 800 C for 4 hrs. 
The TEM micrograph of the powder sample at 100 C in 
fig. (5) is not clear. It shows cloudy appearance support-
ing the XRD pattern of the sample with no intense peak. 
This may be due to the presence of moisture / impurities 
in the sample for 100 C. But the micrograph images at 
600 C shown in fig. (6) are clear and are having cubical 
structure which is supporting our XRD results. 
4. CONCLUSIONS  
 
Nano-sized nickel ferrite particles were successfully 
prepared by co-precipitation method without any capping 
agent. Physically, the color of the precipitated powder 
changes from chocolate-brown to dark-brown and some-
times it becomes black when the sintering temperature is 
increased towards 800 C.The average particle size is 
about 10 nm for powders sintered up to 800 C. The ob-
served results refer to change in phase of NiFe2O4 nano-
particles with increasing sintering temperature. XRD 
peak at different sintering temperatures show crystallini-
ty of the prepared sample increasing with increasing the 
temperature. The cubical structure of the sample is con-
firmed by the TEM. 
 
 
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Synthesis and Characterization of Nickel Ferrite: Role of Sintering Temperature on Structural Parameters

Electronic Sumy State University Institutional Repository

JOURNAL OF NANO- AND ELECTRONIC PHYSICS  ЖУРНАЛ НАНО- ТА ЕЛЕКТРОННОЇ ФІЗИКИ Vol. 6 No 1, 01008(4pp) (2014) Том 6 № 1, 01008(4cc) (2014)   2077-6772/2014/6(1)01008(4) 01008-1  2014 Sumy State University  Synthesis and Characterization of Nickel Ferrite: Role of Sintering Temperature on  Structural Parameters  S.K. Emdadul Islam, Pankaj Sharma*  Department of Physics and Materials Science, Jaypee University of Information Technology,  Waknaghat, Solan, H.P. (173234) India   (Received 30 October 2013; revised manuscript received 04 April 2014; published online 06 April 2014)  We synthesized Nanocrystalline nickel ferrite powder using co-precipitation method and studied the ef-fect of sintering at 100, 400, 600, 800 C on the prepared samples. X-ray diffraction (XRD) and transmis-sion electron microscopy (TEM) were used to characterize the samples. XRD patterns show crystalline na-ture of the sample and the spinel structure of NiFe2O4. Particle size and morphology of the nanocrystalline powders were determined by TEM. The average particle sizes were identified to be 10 nm. Results indicate that the chemical synthesis by co-precipitation method leads to obtain nano crystalline nickel ferrite with controllable particle size.  Keywords: Co-precipitation, Ferrites, Structural parameters.   PACS numbers: 75.50.Gg, 73.63.Bd                                                             * pks_phy@yahoo.co.in 1. INTRODUCTION  Magnetic nanopowders of spinel ferrites (MFe2O4, M  Ni, Co, Mn, Zn etc) are one of the important mate-rials which was first synthesized about 50 years ago [1] and it has got high attention  since few decades due to their useful electromagnetic characteristics for a huge number of technological applications such as infor-mation storage system, radio frequency coils, trans-former, medical field for MRI, sensor, as radar absorb-ing materials (RAM) in military to increase the invisibil-ity to radar etc [2-9]. This is mainly due to their proper-ties are vastly differ from the corresponding bulk mate-rial. The function of these bulk ferrite materials is lim-ited to a few megahertz frequency due to high electrical conductivity and domain wall resonance [10-11]. But in recent time’s electronic industry demand more compact cores for work at higher frequency [12]. This problem of domain wall resonance could be avoided by synthesizing ferrite nanoparticles. In this case domain formation is not favorable energetically below a critical dimension of the particle and it exists as a single domain [13]. Ferrite na-noparticles can be synthesized by wet chemical method such as co-precipitation [14], sol-gel [15], reverse micelles [16], polymeric precursor  and hydrothermal process [17-18]. The formula of the cubic structure of spinel ferrites are described as [A][B]2O4, where A is the tetrahedral and B is octahedral cation sites, in a FCC anion (oxygen) sub-lattice. NiFe2O4 has a normal spinel structure with Ni2 + ions in the A-site and Fe3+ ions in the B-sites [19].  In the present work, we have used the co-precipitation method due to its low cost, tailor made synthesis condi-tions and is very simple method to provide homogeneous powders in greater amount at temperature close to 60 C [20]. Several preparation conditions such as concentration, molar ratio of the cation, pH of the solution and tempera-ture can have an impact on the particle size of the ferrites and their properties [21]. NiFe2O4 powders are sintered at different temperatures. The lattice constant, crystal strain, dislocation density, phase of the ferrites and struc-tural morphology of the nanocrystalline powders were studied. 2. EXPERIMENTAL DETAILS  2.1 Chemicals  Nickel chloride (NiCI2.6H2O); anhydrous ferric chlo-ride (FeCl3); Sodium Hydroxide (NaOH). All chemical were purchased from Merck (AR Grade) and used with-out further purification.   2.2 Synthesis  Nickel ferrite powders with compositions NiFe2O4 have been synthesized via co-precipitation method. First-ly, 0.5M NiCl2.6H20 solution is made by adding 11.88g in 100ml of double distilled water, simultaneously, 1M an-hydrous FeCl3 solution is made by adding 16.22 g in 100 ml of double distilled water. 0.4N NaOH solution (4 g NaOH pallet in 250 ml of distilled water) is used as pre-cipitating agent. 50 ml of nickel chloride solution and 50 ml of ferric chloride solution were mixed and kept at 60 C for 30 minutes. In this mixture, added the boiling NaOH solution under constant stirring till the pH of the solution becomes 12. Nanoferrites are formed by conver-sion of metal salts into hydroxides, followed by transfor-mation of hydroxides into ferrites. The final solution was maintained at 85 C for 80 minutes, this time is sufficient for the transformation of hydroxides into spinel ferrite. Particles were filtered from the solution and were washed several times with double distilled water. Collected parti-cle were then dried at 80 C. The samples were then grinded using mortar pestle and sintered at 100 C, 400 C, 600 C and 800 C for 4 hrs. The precipitated fer-rite is chocolate brown in colour. The overall chemical reaction for the formation of NiFe2O4 may be written by the following way [22-23]:  Ni2 + + 2Fe3 + + 8OH –                   NiFe2O4 + 4H2O  2.3 Characterization  The phase identification of the synthesized powder sample of NiFe2O4 was done by using X-ray diffractom- PANKAJ SHARMA, S.K. EMDADUL ISLAM J. NANO- ELECTRON PHYS. 6, 01008 (2014)   01008-2 eter (XRD) having Cu-Ka radiation. Goniome-ter  PW3050 / 60 (Theta / Theta); Minimum step size 2θ: 0.001; Minimum step size Omega: 0.001. The struc-tural morphology is investigated using transmission electron microscopy (TEM)[Hitachi, H-7500, 40-120 kV operating voltage] at 90 kV.  3. RESULTS AND DISCUSSION  Fig. (1-4) shows the XRD patterns of powder sam-ples after sintering at different temperatures 100 C, 400 C, 600 C and 800 C respectively. XRD data have been used to calculate structural parameters grain size, lattice parameter, strain of the crystal and dislocation density of the prepared sample. The average particle size of the sample was calculated by using Scherrer’s formula [26]:   D  0.9 / cos (1)  where  is full width at half maxima and  is Bragg’s angle. The average strain (Є) of the sample was calculated by Stokes Wilson equation [25]:   Є  /4tan  (2)  Equation is used to calculate the dislocation density [27],   δ  15ε / aD  (3)  where D is average grain size, a is lattice parameter[27]   a  d  (h2 + k2 + l2)0.5 (4)  where d is spacing between two planes. The values of parameters mentioned above are shown in Table 1. With increasing sintering temperature up to 600 C crystal strain and dislocation density de-creases due to an increase in particle size, but at 800 C these parameters increases and particle size decreases. These changes in grain size, crystal strain and disloca-tion density may be due to the crystal deformation after certain temperature. Lattice parameter of the prepared sample decreases with increasing sintering temperature this is may be due to compactness of the lattice in the crystal increases.  10 20 30 40 50 60 70 80020406080100120140160180200intensity2 theta(deg)(311)(222)(400) (440)  Fig. 1 – XRD Pattern for NiFe2O4 at a sintering temperature of 100 C 10 20 30 40 50 60 70 800204060Intensity/a.u4003114406222 Theta(Deg)   Fig. 2 – XRD Pattern for NiFe2O4 at a sintering temperature of 400 C  10 20 30 40 50 60 70 80 900100200300400500intensity2 theta(deg)(220)(311)(222)(400)(511)(440)(5330  Fig. 3 – XRD Pattern for NiFe2O4 at a sintering temperature of 600 C  10 20 30 40 50 60 70 80-1000100200300400500600700intensity2 theta(deg)(311)(220)(400)(222)(422)(511)(440)(533)  Fig. 4 – XRD Pattern for NiFe2O4 at a sintering temperature of 800 C  The characteristic peaks of NiFe2O4 from figure 1-4 confirm the spinel structure of the powder sample and changes phase at different sintering temperature. The reflection peaks for 100 C are corresponding to (311), (222), (400), (440) planes, for 400 C the planes are (311), (400), (440) and (622)  and for 600 C and 800 C planes are (220), (311), (222), (400), (511), (440) and (533) [24]. At 100 C all the characteristic peaks are not intense, two broad lightly intense peaks for (311) and (222) plane are observed. Peak corresponding to (400)    SYNTHESIS AND CHARACTERIZATION OF NICKEL FERRITE… J. NANO- ELECTRON PHYS. 6, 01008 (2014)   01008-3   Fig. 5 – TEM Images for NiFe2O4 at a sintering temperature of 100 C    Fig. 6 – TEM Images for NiFe2O4 at a sintering temperature of 800 C  Table 1 – Lattice Parameter, Strain and Dislocation Density for NiFe2O4 at a sintering temperature of 100, 400, 600 and 800 C  Sintering Temperature (C) Lattice parame-ter (a) (Å) Crystal Strain (Є) Dislocation Density (δ) Particle size (D) (nm) 100 8.3857 6.60  10 – 4 4.5  1014 26 400 8.3354 5.68  10 – 4 2.7  1014 37 600 8.3540 5.18  10 – 4 2.3  1014 42 800 8.3253 8.28  10 – 4 5.3  1014 28  plane is more intense for sintering temperature 400 C in comparison to 100 C. For sintering temperature 600 C, sharp and more intense peaks are obtained for (400) plane along with (220), (511), and (533) planes. Comparing figures (1-4) all peaks become more intense and sharp with increasing sintering temperature i.e., crystalline nature is increased. Since plane (400) has same intensity for sintering temperature 400 C and 600 C so confirms that the phase of the powder crystal is same. But ≥ 600 C highly intense characteristic peaks  PANKAJ SHARMA, S.K. EMDADUL ISLAM J. NANO- ELECTRON PHYS. 6, 01008 (2014)   01008-4 for (311) plane is found. It shows that phase changes above 600 C sintering temperature and also with in-creasing the sintering temperature leads to higher crys-tallinity. The TEM micrographs for NiFe2O4 powder are shown in fig. (5-6). The morphology of the prepared sample is mostly cubical with some agglomeration. The average particle size is estimated to about 10 nm for powder sin-tered at temperatures 100, 400, 600 and 800 C for 4 hrs. The TEM micrograph of the powder sample at 100 C in fig. (5) is not clear. It shows cloudy appearance support-ing the XRD pattern of the sample with no intense peak. This may be due to the presence of moisture / impurities in the sample for 100 C. But the micrograph images at 600 C shown in fig. (6) are clear and are having cubical structure which is supporting our XRD results. 4. CONCLUSIONS   Nano-sized nickel ferrite particles were successfully prepared by co-precipitation method without any capping agent. Physically, the color of the precipitated powder changes from chocolate-brown to dark-brown and some-times it becomes black when the sintering temperature is increased towards 800 C.The average particle size is about 10 nm for powders sintered up to 800 C. The ob-served results refer to change in phase of NiFe2O4 nano-particles with increasing sintering temperature. XRD peak at different sintering temperatures show crystallini-ty of the prepared sample increasing with increasing the temperature. The cubical structure of the sample is con-firmed by the TEM.   REFERENCES  1. Sh. Jabeli Moeen, M.R. Vaezi, A.A. Yousefi, Prog. Color Colorants Coat. 3, 9 (2010). 2. C. Caizer, M. Propovici, C. 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Synthesis and Characterization of Nickel Ferrite: Role of Sintering Temperature on Structural Parameters

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